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A method for synergistic extraction and separation of manganese, calcium and magnesium

An extraction and extraction agent technology, applied in the field of chemical extraction, can solve the problems of incomplete separation of calcium and magnesium, high cost, complicated process, etc., and achieve the effect of good impurity removal effect, low cost and short process.

Active Publication Date: 2021-06-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the defects of high cost, complex process and incomplete separation of calcium and magnesium in the existing methods for removing calcium and magnesium from the acidic manganese-containing solution containing calcium and magnesium, the purpose of the present invention is to provide a method with good separation effect, short flow process, Low-cost collaborative extraction method for separating manganese from calcium and magnesium

Method used

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  • A method for synergistic extraction and separation of manganese, calcium and magnesium
  • A method for synergistic extraction and separation of manganese, calcium and magnesium
  • A method for synergistic extraction and separation of manganese, calcium and magnesium

Examples

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Effect test

Embodiment 1

[0033] A method for synergistically extracting and separating manganese, calcium and magnesium of the present invention, comprising:

[0034] Aqueous phase material solution: lean pyrolusite leaching solution, containing 11.0g / L Mn 2+ , 4.8g / L Mg 2+ , 0.35g / L Ca 2+ , The pH of the feed solution is 3.12.

[0035] Organic phase: Prepare three organic phases with different compositions numbered 1, 2, and 3. The diluent in the organic phase is sulfonated kerosene, and the organic phase No. 1 is sulfonated kerosene with 0.25mol / L phosphoric acid extractant P204 Solution, No. 2 organic phase is the sulfonated kerosene solution of 1mol / L pyridine decanoate, No. 3 is the sulfonated kerosene solution of P204+1mol / L pyridine decanoate that organic phase is 0.25mol / L, utilizes ammonia water to above-mentioned Three kinds of organic phases were subjected to saponification treatment (saponification rate was 60%).

[0036] Extraction and separation: The saponification-treated organic ph...

Embodiment 2

[0041] A method for synergistically extracting and separating manganese, calcium and magnesium of the present invention, comprising:

[0042] The aqueous phase material liquid is the liquid after reducing pyrolusite with waste iron scraps and removing impurities, containing 22.01g / L Mn 2+ , 4.12g / L Mg 2+ , 0.10g / L Ca 2+ , the feed liquid pH is 4, the organic phase is: 0.3mol / L phosphoric acid extractant P507+0.7mol / L aviation kerosene solution of pyridine caprylate, utilize ammonia water to carry out saponification treatment (saponification rate is 60%).

[0043] A separatory funnel was used for single-stage extraction, the extraction ratio was 3 / 1, the extraction mixing time was 10 min, and the temperature was 35°C. The experimental results are shown in Table 2.

[0044] Table 2 Extraction Results

[0045]

[0046] It can be seen from Table 2 that during the extraction process, the single-stage extraction rate of manganese can reach 94.7%, magnesium and calcium are basi...

Embodiment 3

[0048] The aqueous phase feed solution is the same as in Example 2; the organic phase is the Escaid 110 solution of 0.3mol / L phosphoric acid extractant 5709+1mol / L pyridine nonanoate, which is saponified with ammonia water (saponification rate is 60%).

[0049] A separatory funnel was used for single-stage extraction, the extraction ratio was 6 / 1, the extraction mixing time was 10 min, and the temperature was 5°C. The experimental results are shown in Table 3.

[0050] Table 3 Extraction Results

[0051]

[0052] It can be seen from Table 3 that during the extraction process, the single-stage extraction rate of manganese can reach 96.4%, and magnesium and calcium are basically not extracted. The separation coefficients of Mn / Mg and Mn / Ca are respectively above 630 and 220, and the separation effect is good.

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Abstract

The invention discloses a method for synergistic extraction and separation of manganese, calcium and magnesium, comprising: 1) the saponified organic phase containing a synergistic extractant is contacted with an acidic manganese-containing solution containing calcium and magnesium impurities to carry out single-stage or multi-stage countercurrent Extraction; 2) Washing the loaded organic phase with a detergent and contacting the stripping agent with an aqueous solution of inorganic acid for single-stage or multi-stage countercurrent stripping to obtain the stripped organic phase and a high-purity manganese-containing solution; 3) stripping the stripped The organic phase is contacted with the saponification agent for saponification treatment, and the organic phase containing the co-extractant after saponification is obtained, and returned to step 1) for repeated use. The synergistic extractant compounded by phosphoric acid extractant and pyridine carboxylate is used to selectively extract manganese from acidic manganese-containing solution, so as to realize the effective separation of manganese and magnesium ions, calcium ions and other impurity ions, and the loaded organic phase is washed Finally, a mineral acid is used for back extraction to obtain a high-purity manganese-containing solution; the method has a high manganese recovery rate, a good separation effect of manganese and impurities, and is easy to realize industrialization.

Description

technical field [0001] The invention belongs to the technical field of chemical extraction, and in particular relates to a method for synergistic extraction and separation of manganese, calcium and magnesium. Background technique [0002] Manganese sulfate is a very important basic manganese salt. In recent years, due to the development of manganese-based cathode materials, manganese sulfate has been widely used in the battery industry. Battery-grade manganese sulfate has strict requirements on the content of various impurities, especially calcium and magnesium impurities, but the deep removal of calcium and magnesium impurities is still a technical problem in the preparation process of high-purity manganese compounds. At present, the fluoride precipitation method is widely used in industry to remove calcium and magnesium impurities from manganese-containing solutions. This method utilizes the difference between the large solubility product of manganese fluoride and the low ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B26/20C22B26/22C22B47/00C22B3/40
CPCC22B26/20C22B26/22C22B47/00C22B3/409
Inventor 张贵清曾理王应松曹佐英李青刚关文娟肖连生张栋
Owner CENT SOUTH UNIV
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